CN114267756B - A method for preparing light emitting diode epitaxial wafer and epitaxial wafer - Google Patents
A method for preparing light emitting diode epitaxial wafer and epitaxial wafer Download PDFInfo
- Publication number
- CN114267756B CN114267756B CN202111566789.3A CN202111566789A CN114267756B CN 114267756 B CN114267756 B CN 114267756B CN 202111566789 A CN202111566789 A CN 202111566789A CN 114267756 B CN114267756 B CN 114267756B
- Authority
- CN
- China
- Prior art keywords
- layer
- sub
- doped algan
- epitaxial wafer
- type doped
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000013078 crystal Substances 0.000 abstract description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 22
- 238000000034 method Methods 0.000 abstract description 20
- 239000012159 carrier gas Substances 0.000 abstract description 19
- 239000001257 hydrogen Substances 0.000 abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 17
- 229910052786 argon Inorganic materials 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 9
- 230000007547 defect Effects 0.000 abstract description 7
- 230000033001 locomotion Effects 0.000 abstract description 6
- 238000005530 etching Methods 0.000 abstract description 5
- 230000005012 migration Effects 0.000 abstract description 5
- 238000013508 migration Methods 0.000 abstract description 5
- 230000003746 surface roughness Effects 0.000 abstract description 3
- 229910002704 AlGaN Inorganic materials 0.000 description 85
- 238000000137 annealing Methods 0.000 description 18
- 230000000903 blocking effect Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 239000000758 substrate Substances 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 9
- 230000004913 activation Effects 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 125000004429 atom Chemical group 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000002019 doping agent Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 230000007847 structural defect Effects 0.000 description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UOSXPFXWANTMIZ-UHFFFAOYSA-N cyclopenta-1,3-diene;magnesium Chemical compound [Mg].C1C=CC=C1.C1C=CC=C1 UOSXPFXWANTMIZ-UHFFFAOYSA-N 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Led Devices (AREA)
Abstract
本发明公开一种发光二极管外延片制备方法及外延片，在氩气作为载气的条件下生长第一子层，由于氩气具有较大的原子质量，能够提供更高的动量，提高Al原子的横向迁移效率，促进第一子层横向生长，能够降低第一子层以及后续生长的第二子层的表面粗糙度和缺陷密度，提高晶体质量；但是由于第一子层的生长速率较快，容易产生刃位错，通过设置氢气作为载气生长第二子层，由于氢气的分子质量较低，在生长时分子运动活性强，对结晶质量较差的晶体具有刻蚀和重结晶的作用，有助于减小刃位错，进一步提高晶体质量。
The invention discloses a method for preparing a light-emitting diode epitaxial wafer and an epitaxial wafer. A first sublayer is grown under the condition that argon is used as a carrier gas. Since argon has a large atomic mass, it can provide a higher momentum, improve the lateral migration efficiency of Al atoms, promote the lateral growth of the first sublayer, reduce the surface roughness and defect density of the first sublayer and a second sublayer grown subsequently, and improve the crystal quality. However, since the growth rate of the first sublayer is relatively fast, edge dislocations are easily generated. By setting hydrogen as a carrier gas to grow the second sublayer, since the molecular mass of hydrogen is relatively low, the molecular motion activity is strong during growth, and it has the effect of etching and recrystallizing the crystal with poor crystal quality, which helps to reduce edge dislocations and further improve the crystal quality.
Description
Technical Field
The invention relates to the technical field of semiconductor devices, in particular to a preparation method of a light-emitting diode epitaxial wafer and the epitaxial wafer.
Background
In recent years, alGaN materials are paid attention to because of the great application potential of the AlGaN materials in ultraviolet light electric devices, and ultraviolet LEDs have the characteristics of high photon energy, short wavelength, small volume, low power consumption, long service life, environmental friendliness and the like, and have wide application in the fields of high-color-rendering-index white light illumination, high-density optical data storage, sensors, lithography, air purification, environmental protection and the like.
In the conventional AlGaN-based ultraviolet LED structure at present, electrons are easy to overflow into the P-type doped AlGaN layer through the multiple quantum well layers due to the fact that the effective mass of the electrons is smaller and the mobility is higher; therefore, an electron blocking layer doped with an Al component is usually required to be arranged between the multiple quantum well layer and the P-type doped AlGaN layer, and under normal conditions, the higher the Al component in the electron blocking layer is, the better the electron blocking effect is, but as the Al component is more, the lower the transverse migration rate in the epitaxial growth process is due to the higher adhesion coefficient of Al atoms, the high defect density and uneven surface of the electron blocking layer can be caused, so that the morphology of the P-type doped AlGaN layer which grows subsequently can be influenced, and the crystal quality is reduced; meanwhile, the P-type doped AlGaN layer also comprises Al with high component content, so that the activation efficiency of metal particles doped in the P-type doped AlGaN layer is low, the hole concentration is low, and the recombination efficiency of electrons and holes is also low.
Therefore, how to reduce the structural defect of the P-type doped AlGaN layer and improve the crystal quality becomes a problem in the prior art in need of improvement.
Disclosure of Invention
The application aims to provide a preparation method of a light-emitting diode epitaxial wafer and the epitaxial wafer, which are used for solving the problem of how to reduce the structural defect of a P-doped AlGaN layer and improve the crystal quality.
The application adopts the scheme for solving the technical problems that:
In a first aspect, the present application provides a method for preparing an epitaxial wafer of a light emitting diode, which at least includes a substrate and a stacked structure, wherein the stacked structure at least includes a multiple quantum well layer, an electron blocking layer and a P-type doped AlGaN layer, which are arranged from bottom to top, and the method for preparing the P-type doped AlGaN layer includes the following steps:
Argon is used as carrier gas to grow a first P-type doped AlGaN layer to be used as a first sub-layer;
Continuously growing a second P-type doped AlGaN layer on the first sub-layer by taking hydrogen as carrier gas to serve as a second sub-layer; and obtaining the P-type doped AlGaN layer with at least two layers.
In some embodiments of the application, after preparing the second sub-layer, annealing the second sub-layer in a nitrogen atmosphere is further included.
In some embodiments of the application, the growth temperature of the second sub-layer is 1000-1100 ℃.
In some embodiments of the present application, the steps of preparing the first sub-layer and the second sub-layer are repeated, so as to obtain a P-type doped AlGaN layer with a plurality of first sub-layers and a plurality of second sub-layers alternating with each other, wherein each first sub-layer and each second sub-layer are alternately arranged.
In some embodiments of the present application, after the P-doped AlGaN layer is fabricated, further comprising fabricating a contact layer on the P-doped AlGaN layer.
In some embodiments of the present application, before the preparation of the multiple quantum well layer, the method further includes sequentially preparing a buffer layer, an undoped AlGaN layer, and an N-type doped AlGaN layer on the substrate.
In some embodiments of the present application, the mass content ratio of the Al component in the first sub-layer and the second sub-layer is 10% to 50%.
In a second aspect, the present application further provides a light emitting diode epitaxial wafer, at least including a substrate and a stacked structure, where the stacked structure at least includes a multiple quantum well layer, an electron blocking layer, and a P-type doped AlGaN layer disposed from bottom to top, and the P-type doped AlGaN layer includes:
the first sub-layer is made by growing a first P-type doped AlGaN layer by taking argon as carrier gas;
The second sub-layer is arranged on the first sub-layer, and is made by continuously growing a second P-type doped AlGaN layer by taking hydrogen as carrier gas; the P-type doped AlGaN layer is at least provided with a two-layer structure.
In some embodiments of the present application, after the second P-doped AlGaN layer is grown using hydrogen as a carrier gas, annealing is performed in a nitrogen atmosphere to form a second sub-layer.
In some embodiments of the present application, the P-doped AlGaN layer comprises a plurality of alternating first sub-layers and a plurality of second sub-layers, wherein each of the first sub-layers and each of the second sub-layers are alternately arranged.
According to the preparation method of the light-emitting diode epitaxial wafer and the epitaxial wafer, the first sub-layer is grown under the condition that argon is used as carrier gas, and as the argon has larger atomic mass, the higher momentum can be provided, the transverse migration efficiency of Al atoms is improved, the transverse growth of the first sub-layer is promoted, the surface roughness and defect density of the first sub-layer and the second sub-layer which grows subsequently can be reduced, and the crystal quality is improved; however, since the growth rate of the first sub-layer is faster, edge dislocation is easy to generate, and the second sub-layer is grown by setting hydrogen as carrier gas, the molecular mass of the hydrogen is lower, the molecular motion activity is strong during growth, and the etching and recrystallization effects on crystals with poorer crystallization mass are realized, so that the edge dislocation is reduced, and the crystal quality is further improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a diagram of an epitaxial wafer structure of the present invention;
fig. 2 is a step diagram of the epitaxial wafer manufacturing method of the present invention.
Element symbol description:
1-substrate, 2-buffer layer, 3-undoped AlGaN layer, 4-N type doped AlGaN layer, 5-multiple quantum well layer, 6-electron blocking layer, 7-P type doped GaN layer, 8-contact layer, 71-first sub-layer, 72-second sub-layer.
Detailed Description
The technical solutions of the embodiments of the present application will be clearly and fully described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to fall within the scope of the application.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or the inclusion of a number of indicated features. Thus, a feature defining "a first" or "a second" may include, either explicitly or implicitly, one or more of the described features. In the description of the present invention, the meaning of "a plurality" is two or more unless explicitly defined otherwise.
In the application, the term "exemplary" is used to mean "serving as an example, instance, or illustration. Any embodiment described as exemplary in this disclosure is not necessarily to be construed as preferred or advantageous over other embodiments. The following description is presented to enable any person skilled in the art to make and use the application. In the following description, details are set forth for purposes of explanation. It will be apparent to one of ordinary skill in the art that the present application may be practiced without these specific details. In other instances, well-known structures and processes have not been described in detail so as not to obscure the description of the application with unnecessary detail. Thus, the present application is not intended to be limited to the embodiments shown, but is to be accorded the widest scope consistent with the principles disclosed herein.
Particularly for AlGaN-based ultraviolet LEDs, many technical difficulties are faced in development, such as the fact that electrons themselves have smaller effective mass and higher mobility, so that many electrons are easy to overflow into a P layer through a quantum well; with the increase of Al components, the problems of high defect density, uneven surface and the like of an epitaxially grown AlGaN film are easily caused, an AlGaN material with high crystal quality is difficult to obtain, and compared with a GaN material, the AlGaN material with high Al components is more difficult to obtain no matter in N-type doping or P-type doping, especially the doping of P-AlGaN is particularly troublesome, the activation efficiency of a dopant Mg is low, the defect of holes is caused, and the radiation recombination efficiency is reduced; in addition, the quantum efficiency in AlGaN-based ultraviolet LEDs is relatively lower than that of blue-green light emitting diodes, and the performance of the ultraviolet light emitting diodes is severely limited. In order to improve the quantum efficiency of ultraviolet LEDs, it is necessary to prepare highly conductive p-type and n-type AlGaN materials, and epitaxial layers of high crystal quality and quantum well structures of high internal quantum efficiency.
At present, the quantum efficiency in an AlGaN-based ultraviolet LED is relatively lower than that of a blue-green light emitting diode, and the electron-hole radiation recombination efficiency is relatively lower due to the fact that the activation energy of P-type doped AlGaN is high and the hole concentration is not high. When GaN material is adopted for P-type doping, the hole concentration can be improved, but in an ultraviolet LED, gaN absorbs ultraviolet light seriously, so that the extraction efficiency of ultraviolet light is not facilitated; when the AlGaN material is adopted for P-type doping, the absorption of the material to ultraviolet light can be reduced, and the extraction efficiency of ultraviolet light is improved, but the activation energy of the AlGaN material for P-type doping is higher, so that the hole concentration is not high, the luminous efficiency of the ultraviolet LED is reduced, the surface flatness and the crystal quality of an epitaxial layer grown by the AlGaN material are not as high as those of GaN, and the luminous efficiency of the ultraviolet LED is also reduced.
Example 1: referring to fig. 1, the main body of the embodiment is a method for preparing an epitaxial wafer of a light emitting diode, which at least includes a substrate 1 and a stacked structure, wherein the stacked structure at least includes a multi-quantum well layer 5, an electron blocking layer 6 and a P-type doped AlGaN layer arranged from bottom to top, and the method for preparing the P-type doped AlGaN layer includes the following steps: growing a first P-doped AlGaN layer by taking argon as carrier gas as a first sub-layer 71; continuing to grow a second P-doped AlGaN layer as a second sub-layer 72 on the first sub-layer 71 with hydrogen as a carrier gas; and obtaining the P-type doped AlGaN layer with at least two layers. The adhesion coefficient of Al atoms is relatively high, the migration rate is relatively slow during epitaxial growth, and the quality of the obtained epitaxial layer crystal is low; the first sub-layer 71 is grown under the condition that argon is taken as carrier gas, and because the argon has larger atomic mass, the higher momentum can be provided, the transverse migration efficiency of Al atoms is improved, the transverse growth of the first sub-layer 71 is promoted, the surface roughness and defect density of the first sub-layer 71 and the subsequently grown second sub-layer 72 can be reduced, and the crystal quality is improved; however, the epitaxial layer can transversely migrate and combine to form a film on the surface in the growth process; the growth rate of the first sub-layer 71 is faster, edge dislocation is easily generated at the combined interface of the first sub-layer 71 and other layers, and the second sub-layer 72 is grown by setting hydrogen as carrier gas, so that the molecular mass of the hydrogen is lower, the molecular motion activity is strong during growth, and the crystal with poor crystallization quality has the effects of etching and recrystallization, thereby being beneficial to reducing the edge dislocation and further improving the crystal quality.
In some embodiments of the present application, after the second sub-layer 72 is prepared, annealing the second sub-layer 72 in a nitrogen atmosphere is also included. In the traditional preparation process, the contact layer 8 is prepared after the P-type doped AlGaN layer is prepared, and the contact layer 8 is subjected to out-of-furnace unified annealing; in this embodiment, the second sub-layer 72 is annealed in the furnace after being prepared, which is equivalent to uninterrupted annealing, and compared with the annealing outside the furnace, the method can reduce the influence of air outside the furnace and partial vapor on the annealing process of the epitaxial layer; after the second sub-layer 72 is prepared, the growth is interrupted, and only nitrogen is introduced to anneal the second sub-layer 72, so that the purpose is to add annealing treatment to activate holes in the growth process, and compared with the whole annealing process outside the furnace in the traditional process, the annealing process of the second sub-layer 72 in the furnace can fully activate doped Mg, and the hole activation efficiency is higher.
In some embodiments of the present application, the growth temperature of second sub-layer 72 is 1000-1100 ℃. The molecular mass of hydrogen is lower, and the molecular motion activity is strong during growth, particularly the molecular activity is stronger at high temperature, and the hydrogen has intense thermal motion, so that the etching effect can be provided for the crystal with poor crystallization quality, particularly the first sublayer 71 and the second sublayer 72 which are growing can be provided for etching, and the edge dislocation density is reduced by recrystallization after the crystal with edge dislocation defects is etched, so that the crystal quality is further improved. In particular, the growth temperature is 1050-1100 ℃, which can be selected to further enhance the thermal movement of hydrogen. The thickness of the second sub-layer 72 can also be controlled to be 2-5nm, the growth pressure is 50Torr-100Torr, the Mg doping concentration is 1019cm < -3 > -1020cm < -3 >, and the Al component in the AlGaN layer is 0.1-0.5.
In some embodiments of the present application, the steps of preparing the first sub-layer 71 and the second sub-layer 72 are repeated, so as to obtain a multi-layer alternating P-type doped AlGaN layer having a plurality of first sub-layers 71 and a plurality of second sub-layers 72, wherein each first sub-layer 71 and each second sub-layer 72 are alternately arranged. The thickness of the first sub-layer 71 is 2-10nm, the thickness of the second sub-layer 72 is 2-5nm, and the thickness of the whole P-type doped AlGaN layer is 50-200nm; in the whole process of preparing the P-type doped AlGaN layer, the growth temperature is controlled to be between 1000 ℃ and 1100 ℃, the growth pressure interval is 50Torr-100Torr, the Mg doping concentration is between 1019cm -3-1020cm-3, and the Al component in the AlGaN layer is between 0.1 and 0.5.
In some embodiments of the present application, after the P-doped AlGaN layer is prepared, the contact layer 8 is further prepared on the P-doped AlGaN layer. The thickness is between 10nm and 50nm, the growth temperature is between 1000 ℃ and 1100 ℃, the growth pressure is between 50Torr and 100Torr, and the Al component is between 0.0 and 0.3. And the contact layer 8 is an AlGaN contact layer 8.
In some embodiments of the present application, referring to fig. 2, before preparing the multiple quantum well layer 5, the buffer layer 2, the undoped AlGaN layer 3, and the N-doped AlGaN layer 4 are sequentially prepared on the substrate 1. The specific preparation steps also comprise: s1: providing a sapphire Al2O3 substrate 1; s2: growing an AlN buffer layer 2 on the substrate 1 by PVD; s3: the buffer layer 2 is subjected to in-situ annealing treatment in the hydrogen atmosphere in MOCVD; s4: after annealing is completed, an undoped AlGaN layer with the thickness of 1.0 to 3.0 micrometers is grown; s5: after the undoped AlGaN layer is grown, growing a Si doped N-type AlGaN layer; s6: after the growth of the N-type doped AlGaN layer 4 is finished, a multi-quantum well layer 5 is grown; s7: a long AlGaN electron blocking layer 6 after the growth of the multi-quantum well layer 5 is completed; s8: growing a P-type doped AlGaN layer, preparing a periodic structure consisting of a plurality of first sub-layers 71 and a plurality of second sub-layers 72 which are alternated, and annealing after the preparation of each second sub-layer 72 is completed; s9: an AlGaN contact layer 8 is grown on the P-doped GaN layer 7.
In some embodiments of the present application, the mass content ratio of the Al component in the first sub-layer 71 and the second sub-layer 72 is 10% to 50%. More specifically, the mass content of the Al component can be selected to be 50%, and in the preparation process of the application, the mobility of Al can be increased, and even if the mass content of the Al component is selected to be larger, the crystal quality is not reduced.
Example 2: the embodiment also provides a light emitting diode epitaxial wafer, which at least comprises a substrate 1 and a laminated structure, wherein the laminated structure at least comprises a multi-quantum well layer 5, an electron blocking layer 6 and a P-type doped AlGaN layer which are arranged from bottom to top, and the P-type doped AlGaN layer comprises: the first sub-layer 71 is made by growing a first P-doped AlGaN layer with argon as carrier gas; a second sub-layer 72 disposed on the first sub-layer 71, and made by continuously growing a second P-type doped AlGaN layer using hydrogen as a carrier gas; the P-type doped AlGaN layer is at least provided with a two-layer structure.
In some embodiments of the present application, after the second P-doped AlGaN layer is grown using hydrogen as a carrier gas, annealing is performed in a nitrogen atmosphere to form the second sub-layer 72. In some embodiments of the present application, the P-doped AlGaN layer comprises a plurality of alternating first sub-layers 71 and second sub-layers 72, wherein each of the first sub-layers 71 and each of the second sub-layers 72 are alternately arranged.
Example 3: the embodiment particularly discloses a preparation method of a light-emitting diode epitaxial wafer, which is particularly used for preparing an AlGaN-based ultraviolet light-emitting diode epitaxial wafer; the method comprises the following steps:
The first step: adopting (0001) crystal orientation sapphire Al2O3 as a substrate 1;
And a second step of: an AlN buffer layer 2 is grown on the substrate 1 by PVD. The growth temperature is 400-650 ℃, the sputtering power is 2000-4000W, and the pressure is 1-10Torr; growing an AlN buffer layer 2 with the thickness of 15-50 nm;
And a third step of: the buffer layer 2 is subjected to in-situ annealing treatment in the hydrogen atmosphere in MOCVD, the temperature is 1000-1200 ℃, the pressure interval is 150Torr-500Torr, and the time is 5 minutes to 10 minutes;
Fourth step: after annealing is completed, the temperature is regulated to 1050-1200 ℃, an undoped AlGaN layer with the thickness of 1.0-3.0 microns is grown, the growth pressure is 50 Torr-100 Torr, and the Al component is 0.3-0.8;
Fifth step: after the undoped AlGaN layer is grown, a layer of Si doped N-type AlGaN layer is grown, the thickness is between 1.0 and 3.0 microns, the growth temperature is between 1100 and 1200 ℃, the pressure is between 50Torr and 100Torr, the Si doping concentration is between 1019cm -3-1020cm-3, and the Al component is between 0.2 and 0.6;
Sixth step: after the growth of the N-type doped AlGaN layer 4 is finished, a multi-quantum well structure (MQW) is grown, the multi-quantum well layer 5 (MQW) is composed of 5 to 12 periods of GaN/AlGaN, wherein GaN is a well layer, alGaN is a barrier layer, the thickness of a single GaN well layer in the MQW is 2 to 4nm, the growth temperature is 900 to 1000 ℃, and the pressure is 50Torr to 200 Torr; the thickness of the single AlGaN barrier layer is between 8 and 20nm, the growth temperature is between 1000 and 1100 ℃, the growth pressure is between 50Torr and 100Torr, and the Al component is between 0.1 and 0.5;
Seventh step: after the MQW of the multi-quantum well layer 5 grows, the AlGaN electron blocking layer 6EBL grows at the temperature of 1000 ℃ and 1100 ℃, the growth pressure is 50Torr and 100Torr, the growth thickness is 20nm to 100nm, and the Al component is 0.1-0.5;
Eighth step: after the electron blocking layer 6EBL grows, a P-type doped AlGaN layer is grown, wherein the P-type doped AlGaN layer consists of a plurality of first sub-layers 71, second sub-layers 72 and third sub-layers which alternately grow in a single period, the first sub-layers 71 are P-type doped AlGaN sub-layers grown by taking argon (Ar) as carrier gas, the second sub-layers 72 are P-type doped AlGaN sub-layers grown by taking hydrogen (H 2) as carrier gas, the third sub-layers are grown in an interrupted mode, the second sub-layers 72 are annealed by only introducing nitrogen (N 2), the annealing temperature is 800-1000 ℃, the thickness of the first sub-layers 71P-AlGaN is 2-10nm in a single period, the annealing treatment time of the second sub-layers 72P-AlGaN is 2-5nm in a single period, the total thickness of the third sub-layers N 2 in a single period is 5-10s, the growth temperature is between 1000-1100 ℃, the growth pressure interval is 50 r-100Torr, the Mg doping concentration is between 1019cm -3-1020cm-3, and the Al concentration in the single period is 0.0-0.5 m;
Ninth step: alGaN contact layer 8 grows on P-doped GaN layer 7, the thickness is between 10nm and 50nm, the growth temperature interval is 1000-1100 ℃, the growth pressure interval is 50Torr-100Torr, and the Al component is between 0.0-0.3.
Wherein trimethylaluminum (TMAl), trimethylgallium or triethylgallium (TMGa or TEGa), NH3 are used as precursors of group iii source and group v source, respectively, silane and magnesium dicyclopentadiene are used as precursors of N-type dopant and P-type dopant, respectively, and Ar, N 2 and H 2 are used as carrier gases. The AlGaN-based ultraviolet light-emitting diode epitaxial wafer prepared by the embodiment can improve the light extraction efficiency of an ultraviolet LED by improving the content of Al components, and can not reduce the hole concentration and the epitaxial layer crystal quality.
In the foregoing embodiments, the descriptions of the embodiments are focused on, and the portions of one embodiment that are not described in detail in the foregoing embodiments may be referred to in the foregoing detailed description of other embodiments, which are not described herein again.
While the basic concepts have been described above, it will be apparent to those skilled in the art that the foregoing detailed disclosure is by way of example only and is not intended to be limiting. Although not explicitly described herein, various modifications, improvements and adaptations of the application may occur to one skilled in the art. Such modifications, improvements, and modifications are intended to be suggested within the present disclosure, and therefore, such modifications, improvements, and adaptations are intended to be within the spirit and scope of the exemplary embodiments of the present disclosure.
Meanwhile, the present application uses specific words to describe embodiments of the present application. Reference to "one embodiment," "an embodiment," and/or "some embodiments" means that a particular feature, structure, or characteristic is associated with at least one embodiment of the application. Thus, it should be emphasized and should be appreciated that two or more references to "an embodiment" or "one embodiment" or "an alternative embodiment" in various positions in this specification are not necessarily referring to the same embodiment. Furthermore, certain features, structures, or characteristics of one or more embodiments of the application may be combined as suitable.
Similarly, it should be noted that in order to simplify the description of the present disclosure and thereby aid in understanding one or more inventive embodiments, various features are sometimes grouped together in a single embodiment, figure, or description thereof. This method of disclosure does not imply that the subject application requires more features than are set forth in the claims. Indeed, less than all of the features of a single embodiment disclosed above.
In some embodiments, numbers describing the components, number of attributes are used, it being understood that such numbers being used in the description of embodiments are modified in some examples by the modifier "about," approximately, "or" substantially. Unless otherwise indicated, "about," "approximately," or "substantially" indicate that the number allows for a 20% variation. Accordingly, in some embodiments, numerical parameters set forth in the specification and claims are approximations that may vary depending upon the desired properties sought to be obtained by the individual embodiments. In some embodiments, the numerical parameters should take into account the specified significant digits and employ a method for preserving the general number of digits. Although the numerical ranges and parameters set forth herein are approximations in some embodiments for use in determining the breadth of the range, in particular embodiments, the numerical values set forth herein are as precisely as possible.
Each patent, patent application publication, and other material, such as articles, books, specifications, publications, documents, etc., cited herein is hereby incorporated by reference in its entirety except for any application history file that is inconsistent or otherwise conflict with the present disclosure, which places the broadest scope of the claims in this application (whether presently or after it is attached to this application). It is noted that the description, definition, and/or use of the term in the appended claims controls the description, definition, and/or use of the term in this application if the description, definition, and/or use of the term in the appended claims does not conform to or conflict with the present disclosure.
The foregoing has outlined the detailed description of the embodiments of the present application, and the detailed description of the principles and embodiments of the present application is provided herein by way of example only to facilitate the understanding of the method and core concepts of the present application; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present application, the present description should not be construed as limiting the present application.
Claims (10)
1. The preparation method of the light-emitting diode epitaxial wafer is characterized by at least comprising a substrate and a laminated structure, wherein the laminated structure at least comprises a multi-quantum well layer, an electron blocking layer and a P-type doped AlGaN layer which are arranged from bottom to top, and the preparation method of the P-type doped AlGaN layer comprises the following steps:
Argon is used as carrier gas to grow a first P-type doped AlGaN layer to be used as a first sub-layer;
and continuously growing a second P-type doped AlGaN layer on the first sub-layer by taking hydrogen as carrier gas as a second sub-layer.
2. The method of claim 1, further comprising annealing the second sub-layer in a nitrogen atmosphere after the second sub-layer is prepared.
3. The method of claim 1, wherein the second sub-layer has a growth temperature of 1000-1100 ℃.
4. The method for preparing a light-emitting diode epitaxial wafer according to claim 2, wherein the steps of preparing the first sub-layer and the second sub-layer are repeated to obtain a P-type doped AlGaN layer with a plurality of first sub-layers and a plurality of second sub-layers which are alternately arranged, and each first sub-layer and each second sub-layer are alternately arranged.
5. The method of claim 1, further comprising forming a contact layer on the P-doped AlGaN layer after forming the P-doped AlGaN layer.
6. The method of claim 1, further comprising sequentially forming a buffer layer, an undoped AlGaN layer, and an N-doped AlGaN layer on the substrate before forming the multiple quantum well layer.
7. The method for manufacturing a light-emitting diode epitaxial wafer according to claim 1, wherein the mass content ratio of the Al component in the first sub-layer and the second sub-layer is 10% -50%.
8. The light-emitting diode epitaxial wafer is characterized by at least comprising a substrate and a laminated structure, wherein the laminated structure at least comprises a multi-quantum well layer, an electron blocking layer and a P-type doped AlGaN layer which are arranged from bottom to top, and the P-type doped AlGaN layer comprises:
the first sub-layer is made by growing a first P-type doped AlGaN layer by taking argon as carrier gas;
The second sub-layer is arranged on the first sub-layer, and is made by continuously growing a second P-type doped AlGaN layer by taking hydrogen as carrier gas; the P-doped AlGaN layer comprises at least one first sub-layer and at least one second sub-layer.
9. The led epitaxial wafer of claim 8, wherein hydrogen is used as a carrier gas to grow the second P-doped AlGaN layer and then annealed in a nitrogen atmosphere to form the second sub-layer.
10. The light emitting diode epitaxial wafer of claim 8, wherein the P-doped AlGaN layer comprises a plurality of alternating first sub-layers and a plurality of second sub-layers, wherein each of said first sub-layers and each of said second sub-layers are alternately disposed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111566789.3A CN114267756B (en) | 2021-12-20 | 2021-12-20 | A method for preparing light emitting diode epitaxial wafer and epitaxial wafer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111566789.3A CN114267756B (en) | 2021-12-20 | 2021-12-20 | A method for preparing light emitting diode epitaxial wafer and epitaxial wafer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114267756A CN114267756A (en) | 2022-04-01 |
| CN114267756B true CN114267756B (en) | 2024-09-10 |
Family
ID=80828157
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111566789.3A Active CN114267756B (en) | 2021-12-20 | 2021-12-20 | A method for preparing light emitting diode epitaxial wafer and epitaxial wafer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114267756B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114695612B (en) * | 2022-06-01 | 2022-08-26 | 江西兆驰半导体有限公司 | Gallium nitride-based light emitting diode epitaxial structure and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441065A (en) * | 2013-08-14 | 2013-12-11 | 西安交通大学 | Method for preparing P-type ohmic contact layer of high Al content AlGaN material and application of P-type ohmic contact layer |
| CN103515495A (en) * | 2013-09-13 | 2014-01-15 | 华灿光电股份有限公司 | GaN-base light-emitting diode chip growing method |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3244980B2 (en) * | 1995-01-06 | 2002-01-07 | 株式会社東芝 | Method for manufacturing semiconductor device |
| JP5179055B2 (en) * | 2006-12-26 | 2013-04-10 | 昭和電工株式会社 | Group III nitride semiconductor manufacturing method, group III nitride semiconductor light emitting device manufacturing method, group III nitride semiconductor light emitting device, and lamp |
| JP5049659B2 (en) * | 2007-06-11 | 2012-10-17 | 昭和電工株式会社 | Group III nitride semiconductor manufacturing method, group III nitride semiconductor light emitting device manufacturing method, group III nitride semiconductor light emitting device, and lamp |
| CN104620366B (en) * | 2012-09-12 | 2017-09-26 | 松下知识产权经营株式会社 | Semiconductor device |
| JP2015167177A (en) * | 2014-03-04 | 2015-09-24 | 豊田合成株式会社 | Group III nitride semiconductor light emitting device manufacturing method |
| CN105633223B (en) * | 2015-12-31 | 2018-10-09 | 华灿光电(苏州）有限公司 | Semiconductor devices in AlGaN templates, the preparation method of AlGaN templates and AlGaN templates |
| CN106449905A (en) * | 2016-10-27 | 2017-02-22 | 湘能华磊光电股份有限公司 | A LED growth method to improve the quality of epitaxial crystal |
| CN106835268A (en) * | 2017-01-17 | 2017-06-13 | 苏州瑞而美光电科技有限公司 | A kind of preparation method of group III-nitride substrate |
| RU2673515C2 (en) * | 2017-02-02 | 2018-11-27 | Общество С Ограниченной Ответственностью "Монолюм" | Gases to the reactor supplying method for the group iii metals nitrides based epitaxial structures growing and device for its implementation |
-
2021
- 2021-12-20 CN CN202111566789.3A patent/CN114267756B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441065A (en) * | 2013-08-14 | 2013-12-11 | 西安交通大学 | Method for preparing P-type ohmic contact layer of high Al content AlGaN material and application of P-type ohmic contact layer |
| CN103515495A (en) * | 2013-09-13 | 2014-01-15 | 华灿光电股份有限公司 | GaN-base light-emitting diode chip growing method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114267756A (en) | 2022-04-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101689586B (en) | Nitride semiconductor light emitting element and method for manufacturing nitride semiconductor | |
| CN102368519B (en) | A kind of method improving semiconductor diode multiple quantum well light emitting efficiency | |
| JP2001160627A (en) | Group III nitride compound semiconductor light emitting device | |
| JP4948720B2 (en) | Nitrogen compound semiconductor laminate, light emitting element, optical pickup system, and method for producing nitrogen compound semiconductor laminate. | |
| EP2270879B1 (en) | Nitride semiconductor light emitting element and manufacturing method thereof | |
| JP2001160627A5 (en) | ||
| CN115472718B (en) | Light emitting diode epitaxial wafer, preparation method thereof and light emitting diode | |
| CN115714155A (en) | Deep ultraviolet light emitting diode epitaxial wafer, preparation method thereof and deep ultraviolet light emitting diode | |
| CN117253948B (en) | Light-emitting diode epitaxial wafer, preparation method thereof and light-emitting diode | |
| CN109860353B (en) | GaN-based light emitting diode epitaxial wafer and preparation method thereof | |
| CN116072780B (en) | Light-emitting diode epitaxial wafer, preparation method thereof and light-emitting diode | |
| CN118572003B (en) | Light-emitting diode epitaxial wafer and preparation method thereof, and light-emitting diode | |
| CN114497303B (en) | Long-wavelength LED homoepitaxy structure, preparation method and application thereof | |
| CN116581216B (en) | Light-emitting diode epitaxial wafer and preparation method thereof, light-emitting diode | |
| CN109786513B (en) | Epitaxial wafer of light emitting diode and manufacturing method thereof | |
| WO2009142265A1 (en) | Iii nitride semiconductor light emitting element and method for manufacturing the same, and lamp | |
| CN117199203A (en) | Light-emitting diode epitaxial wafer, preparation method thereof and light-emitting diode | |
| CN117810324A (en) | Light-emitting diode epitaxial wafer, preparation method thereof and light-emitting diode | |
| CN114267756B (en) | A method for preparing light emitting diode epitaxial wafer and epitaxial wafer | |
| JP2001077413A (en) | Group iii nitride semiconductor light-emitting element and manufacture thereof | |
| CN113707772A (en) | Manufacturing method of LED epitaxial wafer for reducing dislocation density | |
| CN116072784B (en) | Deep ultraviolet light-emitting diode epitaxial wafer and its preparation method, LED | |
| CN116014041B (en) | Light-emitting diode epitaxial wafer, preparation method thereof and light-emitting diode | |
| CN109860341B (en) | GaN-based light emitting diode epitaxial wafer and preparation method thereof | |
| CN109461802B (en) | GaN-based light emitting diode epitaxial wafer and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |